Bobebt b



ROBERT 13. 1.3330, 0F ELIZABETH, llElV JERSEY; A$SIGNOR TO STANDARD OIL DEVELQP- terms rice MENU. COMPANY, A CORPORATION OF DELAWARE PROCESS FOR THE FORMATION" OF ALCOHOLS No Drawing.

The present invention relates to the formation of alcohols from olefin hydrocarbons and more specifically comprises an improved method for hydrolyzing alkyl sulphates whereby a larger yield of alcohols is obtained and the product is superior as to purity. My improved process will be fully understood from the following description.

In the production of alcohols from olefin hydrocarbons according to the method of Ellis et al. described and patented in the Letters Patent U. S. 1,4865% of March 11, 1924;, olefin containing hydrocarbons either in gas or liquid phase are contacted with sulphuric acid under sulphating conditions whereby alkyl sulphates are formed. Water is then added to dilute the mass with the result that the sulphates are hydrolyzed forming alcohols and sulphuric acid. Tt is come monly the practice to dilute the acid liquor to a 10 or 18 1%. and it is observedthat two layers are formed. and generally foul smelling due to impurities and it is found to contain a considerable proportion of secondary alcohols higher than isopropyl; Tt is dirlicult, hm ever, to recover these higher alcohols in a pure state. The acid layer which also contains the majority of the isopropyl alcohol is distilled in lead stills or otherwise from which the alcohol is obtained as a distillate and the sulphuric acid residue may be reconcentrated to the proper degree for reacting with a further quantity of olefins.

I have found it to be of reat advantage to dilute the acid liquor in two stages. ll ater is first added until an oily layer separates and it is found on analysis that the oily material contains little or no alcohol hut is rich in the foul smelling impurities which arevery objectionable in the finished product. The quantity of water addec may not be sharply or accurately controlled for there is a considerable range of dilution in which the oily material will separate with little or no alcohol. For example dilutions to a concentration of about 45% by weight of acid based merely on the acid and water and neglecting any olefins and alcohols, allows the oily layer to separate and further dilution to about 30% strength The upper layer is oily Application filed. March 9, 1929. Serial No. 345,891.

on the same basis results in only a negligibly small-loss of alcohols in the oily layer. These limits may also be expressed on the gravity of the aqueous layer but they are less rigid since the amount of olefins or alcohols greatly affect the gravity of the aqueous layer. However, the limits are approximately 45 B. and 22 B. j

The oily layer is then removed by the decantation and discarded. The aqueous layor is then diluted in the second stage to an acid 'strength of 15 to 17% H 80 by weight based as above only on the water and acid present. This dilution liberates a layer which is rich in alcohols higher than isopropyl and secondary butyl alcohols. The layer is decanted and the various components may be separated and purified by any preferredmethod or may be sold as a mixture of higher alcohols, secondary amyl, hexyl, heptyl and the like although a small quantity of the lower alcohols may be present.

The dilute aqueous acid layer is distilled as before for recovery of the alcohols, principally isopropyl and secondary butyl although a small amount of high alcohols may be present. The alcohol may be purified in any preferred manner by treating agents sech as acids, alkali, activated clay, or the li re.

In the following claims the terms acid strength denotes the presence of sulphuric acid by weight calculated on the water and acid only and neglecting the alcohol or olefins present, for example 45% indicates a ratio of 9 parts of acid to 11 parts of water by weight.

My process may be carried out in any convenient form of apparatus adopted to with stand the corrosive action of the acid as will be understood. My invention is not be limited by anytheory of the chemical reactions nor by any example which may be given -merely for purposes of illustration, but only der sulphating conditions, comprising adding Water to the liquor until an oily layer separates, decanting the layer, and recovering alcohol from the aqueous layer.

5 2. A process according to claim 1 in which the addition of Water is added in such amounts as to produce an aqueous layer of about 3045% by Weight acid strength When only the amounts of Water and acid are taken into consideration.

ROBERT B. LEBO. 

